Methyl iodide → 2,6-dichloro-3-methyl-N-[2-[5-(methylthio)-1,3,4-oxadiazol-2-yl]phenyl]benzenamine

HRID 2211185ノート

反応式

HRID 2211185 の反応式
[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[C:4]([Cl:9])[C:3]=1[NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17]1[O:21][C:20](=[S:22])[NH:19][N:18]=1.[OH-].[Na+].I[CH3:26]>CO>[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[C:4]([Cl:9])[C:3]=1[NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17]1[O:21][C:20]([S:22][CH3:26])=[N:19][N:18]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 99284195-[2-(2,6-Dichloro-3-methyl-phenylamino)-phenyl]-[1,3,4]oxadiazole-2-thiol

生成物 1

HCID 193757012,6-dichloro-3-methyl-N-[2-[5-(methylthio)-1,3,4-oxadiazol-2-yl]phenyl]benzenamine収率 86.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a room temperature suspension of 5-[2-[(2,6-dichloro-3-methylphenyl)amino]phenyl]-1,3,4-oxadiazole-2(3H)-thione (1.706 g, 4.85 mmoles) in 70 ml of methanol is added dropwise 5.0 ml of 1.0N sodium hydroxide. The clear pale yellow solution is stirred at room temperature for 10 minutes. Iodomethane (320.0 μl, 5.13 mmoles) is added dropwise, and stirring is continued for six hours. The white solid is collected by filtration and dried in vacuo overnight at 60° C. to provide 1.530 g (86%) of 2,6-dichloro-3-methyl-N-[2-[5-(methylthio)-1,3,4-oxadiazol-2-yl]phenyl]benzenamine, mp 170°-171° C.

後処理

  1. stirringstirring
  2. waitis continued for six hours
  3. filtrationThe white solid is collected by filtration
  4. customdried in vacuo overnight at 60° C.

出典と根拠

ORDレコード
ord-9c366ee8bb21425f82de0c3bb8529208
出典データセット
uspto-grants-1995_10
特許番号
US05462952

反応ノート

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